CN105948095B - The method that regular hexagon calcium carbonate nano crystal grain is prepared based on reverse microemulsion - Google Patents
The method that regular hexagon calcium carbonate nano crystal grain is prepared based on reverse microemulsion Download PDFInfo
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- CN105948095B CN105948095B CN201610589834.XA CN201610589834A CN105948095B CN 105948095 B CN105948095 B CN 105948095B CN 201610589834 A CN201610589834 A CN 201610589834A CN 105948095 B CN105948095 B CN 105948095B
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 57
- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 39
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 29
- 239000002159 nanocrystal Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 30
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 25
- 239000011575 calcium Substances 0.000 claims abstract description 25
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- 239000004064 cosurfactant Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 14
- 229910001424 calcium ion Inorganic materials 0.000 claims description 14
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 5
- AMJQWGIYCROUQF-UHFFFAOYSA-N calcium;methanolate Chemical compound [Ca+2].[O-]C.[O-]C AMJQWGIYCROUQF-UHFFFAOYSA-N 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 4
- 230000001186 cumulative effect Effects 0.000 claims description 4
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003995 emulsifying agent Substances 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 2
- JHLCADGWXYCDQA-UHFFFAOYSA-N calcium;ethanolate Chemical compound [Ca+2].CC[O-].CC[O-] JHLCADGWXYCDQA-UHFFFAOYSA-N 0.000 claims description 2
- MMLSWLZTJDJYJH-UHFFFAOYSA-N calcium;propan-2-olate Chemical compound [Ca+2].CC(C)[O-].CC(C)[O-] MMLSWLZTJDJYJH-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 10
- 239000008346 aqueous phase Substances 0.000 abstract description 5
- 239000012071 phase Substances 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 230000001276 controlling effect Effects 0.000 abstract description 2
- 239000002537 cosmetic Substances 0.000 abstract description 2
- 238000004146 energy storage Methods 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract description 2
- 239000004575 stone Substances 0.000 abstract description 2
- 239000011232 storage material Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract 1
- 230000001476 alcoholic effect Effects 0.000 abstract 1
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 238000000280 densification Methods 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 abstract 1
- NVXIEDHPFHVZTC-UHFFFAOYSA-N calcium;methanol Chemical compound [Ca].OC NVXIEDHPFHVZTC-UHFFFAOYSA-N 0.000 description 9
- 239000007788 liquid Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of method that regular hexagon calcium carbonate nano crystal grain is prepared based on reverse microemulsion, the reverse microemulsion in this method is main by (NH4)2CO3The aqueous solution or NH4HCO3The aqueous solution, compound surfactant and cosurfactant composition (it is required that HLB value=3.0~7.0), using the alcoholic solution of organic calcium as calcium source, by regulating and controlling W/O systems aqueous phase, the volume ratio of oil phase and the molar concentration rate for changing additional particle solution and aqueous phase particle solution, the regular hexagon calcium carbonate crystal grain that the length of side is less than 25nm is prepared at normal temperatures and pressures.Regular hexagon cium carbonate nanoparticles prepared by the present invention have that size is small, specific surface area big, surface can it is high, there is higher activity, densification speed to reduce the performances such as sintering temperature soon; the fields such as energy storage material, chemical catalysis, medical science, cosmetics, the manufacture of best bright finish structure member, stone cultural artifact protection and reparation are can be widely applied to, are the inorganic material that a class has wide use space.
Description
Technical field
The invention belongs to the synthesis technical field of mineral-type materials, and in particular to one kind prepares positive six using reverse microemulsion
The method of side shape nano-calcium carbonate.
Background technology
Reverse microemulsion method is that what is just come into vogue in recent years prepare the new method of material, by seeking one or more
The preparation of microemulsion synthesizes the particle of different sizes and shapes, so that the associated materials of property needed for obtaining people.Micro emulsion
Liquid is Thermodynamically stable, isotropism, appearance transparent or the translucent dispersion of two kinds of immiscible liquid formation, micro-
It is that the droplets of the one or two kinds of liquid stablized by surfactant interface film is constituted in sight.In configuration aspects, microemulsion
Have O/W and W/O two types, the former is that oil phase is dispersed in aqueous phase, the latter be Aqueous dispersions in oil phase, it is different types of micro-
Emulsion is mainly what is determined by the HLB value caused by surfactant.The particle of dispersed phase is generally spherical, and radius is small
(10~100nm), is thermodynamic stable system.Because dispersate spot size is small and uniform, so working as has external particle in physics
Under effect when " invasion ", blended inside two kinds of particles, under the even phase separation surrounded outside, particle size after mixing,
Shape is hardly changed, and now " new " particle has reformed into microreactor, and corresponding particle is just generated in reactor.Print
Three scientists such as degree Ashok K.Ganguli have delivered the summary up to page 12 on Chemical Society Reviews
Article, describes the property and purposes of microemulsion in detail.At present, using microemulsion reaction methods material be concentrated mainly on silicon materials with
And in terms of the catalyst of battery, and obtaining good effect, such as Hunan University Tan Weihong professors team utilizes positive silicic acid second
Ester (TEOS) decomposition, W/O systems have synthesized the silicon dioxide microsphere of nano-grade size.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of utilization isotropism, property stable reverse microemulsion
And active organic calcium, side of the length of side for 15~25nm regular hexagon calcium carbonate nano crystal grain is synthesized at normal temperatures and pressures
Method.
The technical scheme that solution above-mentioned technical problem is used is made up of following step：
1st, W/O reverse microemulsions are prepared
By (NH4)2CO3The aqueous solution or NH4HCO3The aqueous solution with ammoniacal liquor adjust pH value to 8~10, be then added to hexamethylene,
In compound surfactant, the mixed liquor of cosurfactant, it is well mixed, stands, take supernatant, obtain W/O Microemulsions
Liquid, is counted using the cumulative volume of W/O reverse microemulsions as 100%, wherein (NH4)2CO3The aqueous solution or NH4HCO3The aqueous solution accounts for 1%~
4%th, compound surfactant accounts for 0.5%~1.5%, cosurfactant and accounts for 1%~3%, and remaining is hexamethylene, the body of ammoniacal liquor
Product is ignored.
2nd, calcium source solution is prepared
Purity is scattered in deionized water for more than 99% organic calcium, obtain calcium ion concentration for 0.005~
0.08mol/L calcium source solution, wherein during described organic calcium is calcium methoxide, calcium ethoxide, calcium isopropoxide, 2-methyl cellosolve calcium
Any one.
3rd, regular hexagon calcium carbonate nano crystal grain is prepared
Under agitation, the calcium source solution in step 2 is added dropwise in the W/O reverse microemulsions of step 1, controlled
The mol ratio of carbanion and calcium ion in calcium source solution is 30 in W/O reverse microemulsions:0.5~8, after completion of dropping, from
The heart is separated, ultra-pure water centrifuge washing 2~4 times again of lower floor's suspension, is dried, is obtained regular hexagon calcium carbonate nano crystal grain.
In above-mentioned preparation W/O reverse microemulsion steps 1, counted using the cumulative volume of W/O reverse microemulsions as 100%, preferably
(NH4)2CO3The aqueous solution or NH4HCO3The aqueous solution accounts for 2%~3%, compound surfactant and accounts for 0.8%~1.0%, helps surface to live
Property agent accounts for 1.5%~2.0%, and remaining is hexamethylene, and the volume of ammoniacal liquor is ignored.
Above-mentioned compound surfactant is that the volume ratio of Emulsifier EL-60 and Span-80 is 6:4~7:3 mixing
Thing, described cosurfactant is any one in ethanol, n-butanol, isobutanol, n-amyl alcohol.
In above-mentioned preparation calcium source solution step 2, the concentration of calcium ion is 0.01~0.04mol/L preferably in calcium source solution.
It is above-mentioned to prepare in regular hexagon calcium carbonate nano crystal grain step 3, preferably in W/O reverse microemulsions carbanion with
The mol ratio of calcium ion is 30 in calcium source solution:1~4.
The present invention " microreactor " is done with W/O system microemulsions, due to the system have Thermodynamically stable, isotropism,
The advantages of appearance transparent and small size, the present invention is by regulating and controlling W/O systems aqueous phase, the volume ratio of oil phase, and the additional matter of change
The molar concentration rate of point solution and aqueous phase particle solution, is prepared into the regular hexagon carbonic acid that the length of side is less than 25nm at normal temperatures and pressures
Calcium crystal grain, and prepared calcium carbonate shape is regular, marshalling, size are minimum and controllable, with specific surface area is big, surface
Energy is high, have higher activity, fine and close speed to reduce the performances such as sintering temperature soon, can be widely applied to energy storage material, chemistry and urges
The fields such as change, medical science, cosmetics, the manufacture of best bright finish structure member, stone cultural artifact protection and reparation, are that a class has wide make
With the inorganic material in space.
Brief description of the drawings
Fig. 1 is the XRD spectra of regular hexagon calcium carbonate nano crystal grain prepared by embodiment 1.
Fig. 2 is the Flied emission transmission electron microscope photo of regular hexagon calcium carbonate nano crystal grain prepared by embodiment 1.
Fig. 3 is Fig. 2 partial enlarged drawing.
Fig. 4 is the Flied emission transmission electron microscope photo of regular hexagon calcium carbonate nano crystal grain prepared by embodiment 2.
Fig. 5 is the Flied emission transmission electron microscope photo of regular hexagon calcium carbonate nano crystal grain prepared by embodiment 3.
Embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not only limited
In these embodiments.
Embodiment 1
1st, W/O reverse microemulsions are prepared
200mL hexamethylenes are added to after 1.2mL Emulsifier EL-60s, 0.8mL Span-80s, 3mL ethanol are well mixed
In；To (the NH that 5mL mass fractions are 14.3%4)2CO3Ammoniacal liquor is added dropwise in the aqueous solution, it is 9.4 to adjust its pH value, is then dripped
It is added in above-mentioned hexamethylene, stirs, stands 2 hours, take supernatant, obtain W/O reverse microemulsions.
2nd, calcium source solution is prepared
By 0.204g purity for more than 99% calcium methoxide ultrasonic disperse in 50mL deionized waters, obtain calcium ion concentration
For 0.04mol/L methanol calcium solution.
3rd, regular hexagon calcium carbonate nano crystal grain is prepared
Under agitation, 5mL is taken to be added dropwise to the W/O reverse microemulsions of step 1 the methanol calcium solution in step 2
In, the mol ratio of carbanion and calcium ion in methanol calcium solution is 30 in W/O reverse microemulsions:2, after completion of dropping, from
The heart is separated, ultra-pure water centrifuge washing 2~4 times again of lower floor's suspension, 40 DEG C of dryings, obtains regular hexagon calcium carbonate nano brilliant
Grain.
Products obtained therefrom uses D/Max-3cX types x-ray diffractometer (XRD), Tecnai G2F20 type Flied emission transmitted electrons
Microscope is characterized respectively, as a result sees Fig. 1~3.As seen from Figure 1, products obtained therefrom is calcium carbonate.From Fig. 2 and 3, gained
Calcium carbonate is in regular hexagon, and marshalling, and the length of side of single regular hexagon is 15~20nm.
Embodiment 2
The step 1 of the present embodiment is same as Example 1；It is more than 99% by 0.102g purity in the step 2 of the present embodiment
Calcium methoxide ultrasonic disperse in 50mL deionized waters, obtain calcium ion concentration be 0.02mol/L methanol calcium solution；This implementation
Example step 3 in, under agitation, by the methanol calcium solution in step 2 take 5mL be added dropwise to step 1 W/O it is reversely micro-
In emulsion, the mol ratio of carbanion and calcium ion in methanol calcium solution is 30 in W/O reverse microemulsions:1, completion of dropping
Afterwards, centrifuge, lower floor's suspension ultra-pure water centrifuge washing 2~4 times again, 40 DEG C of dryings obtain regular hexagon calcium carbonate and received
Rice crystal grain.From fig. 4, it can be seen that gained calcium carbonate is in regular hexagon, and marshalling, the length of side of single regular hexagon for 15~
25nm。
Embodiment 3
The step 1 of the present embodiment is same as Example 1；It is more than 99% by 0.306g purity in the step 2 of the present embodiment
Calcium methoxide ultrasonic disperse in 50mL deionized waters, obtain calcium ion concentration be 0.06mol/L methanol calcium solution；This implementation
Example step 3 in, under agitation, by the methanol calcium solution in step 2 take 5mL be added dropwise to step 1 W/O it is reversely micro-
In emulsion, the mol ratio of carbanion and calcium ion in methanol calcium solution is 30 in W/O reverse microemulsions:3, completion of dropping
Afterwards, centrifuge, lower floor's suspension ultra-pure water centrifuge washing 2~4 times again, 40 DEG C of dryings obtain regular hexagon calcium carbonate and received
Rice crystal grain.As seen from Figure 5, gained calcium carbonate is in regular hexagon, and marshalling, the length of side of single regular hexagon for 15~
20nm。
Claims (4)
1. a kind of method that regular hexagon calcium carbonate nano crystal grain is prepared based on reverse microemulsion, it is characterised in that it is by following steps
Rapid composition：
(1) W/O reverse microemulsions are prepared
By (NH4)2CO3The aqueous solution or NH4HCO3The aqueous solution adjusts pH value to 8~10 with ammoniacal liquor, is then added to hexamethylene, compounding
In surfactant, the mixed liquor of cosurfactant, it is well mixed, stands, take supernatant, obtain W/O reverse microemulsions, with
The cumulative volume of W/O reverse microemulsions is 100% meter, wherein (NH4)2CO3The aqueous solution or NH4HCO3The aqueous solution accounts for 1%~4%, answered
0.5%~1.5%, cosurfactant is accounted for surfactant and accounts for 1%~3%, remaining is hexamethylene, and the volume of ammoniacal liquor is ignored
Disregard；
Above-mentioned compound surfactant is that the volume ratio of Emulsifier EL-60 and Span-80 is 6:4~7:3 mixture；
Described cosurfactant is any one in ethanol, n-butanol, isobutanol, n-amyl alcohol；
(2) calcium source solution is prepared
Purity is scattered in deionized water for more than 99% organic calcium, calcium ion concentration is obtained for 0.005~0.08mol/L
Calcium source solution, wherein described organic calcium is any one in calcium methoxide, calcium ethoxide, calcium isopropoxide, 2-methyl cellosolve calcium
Kind；
(3) regular hexagon calcium carbonate nano crystal grain is prepared
Under agitation, the calcium source solution in step (2) is added dropwise in the W/O reverse microemulsions of step (1), controlled
The mol ratio of carbanion and calcium ion in calcium source solution is 30 in W/O reverse microemulsions:0.5~8, after completion of dropping, from
The heart is separated, ultra-pure water centrifuge washing 2~4 times again of lower floor's suspension, is dried, is obtained regular hexagon calcium carbonate nano crystal grain.
2. the method according to claim 1 that regular hexagon calcium carbonate nano crystal grain is prepared based on reverse microemulsion, it is special
Levy and be：In W/O reverse microemulsions step (1) is prepared, counted using the cumulative volume of W/O reverse microemulsions as 100%, wherein
(NH4)2CO3The aqueous solution or NH4HCO3The aqueous solution accounts for 2%~3%, compound surfactant and accounts for 0.8%~1.0%, helps surface to live
Property agent accounts for 1.5%~2.0%, and remaining is hexamethylene, and the volume of ammoniacal liquor is ignored.
3. the method according to claim 1 that regular hexagon calcium carbonate nano crystal grain is prepared based on reverse microemulsion, it is special
Levy and be：In calcium source solution step (2) is prepared, the concentration of calcium ion is 0.01~0.04mol/L in described calcium source solution.
4. the method according to claim 1 that regular hexagon calcium carbonate nano crystal grain is prepared based on reverse microemulsion, it is special
Levy and be：In regular hexagon calcium carbonate nano crystal grain step (3) is prepared, control W/O reverse microemulsions in carbanion with
The mol ratio of calcium ion is 30 in calcium source solution:1~4.
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| CN103232051A (en) * | 2013-04-24 | 2013-08-07 | 陕西科技大学 | Preparation method of ultrafine porous calcium carbonate microsphere |
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| CN102583481A (en) * | 2012-01-18 | 2012-07-18 | 兰州交通大学 | Method for preparing spherical nanometer calcium carbonate particles of different grain diameters by reverse microemulsion method |
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| "两亲分子辅助下的无机盐纳米材料的制备";俞冬;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20081115(第11期);B020-54正文第15-17页 * |
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